反应详情

2-Nitrodiphenyl ether (16 g, 74 mmol) in methanol (250 ml) was shaken with palladium on charcoal (1.6 g) under an atmosphere of hydrogen at 20-50° C. for 30 min. There was a rapid uptake of hydrogen and a detectable exotherm 20-50° C. with the temperature rapidly rising before cooling. Shaking was stopped for short periods to control the temperature from rising above 50° C. The reaction was then filtered through celite and concentrated in high vacuum to give 2-aminodiphenyl ether as an oil (13.5 g, 72.9 mmole, 98%) that crystallized on standing to give a buff solid.

1. customa detectable exotherm 20-50° C.
2. temperaturebefore cooling
3. waitwas stopped for short periods
4. customfrom rising above 50° C
5. filtrationThe reaction was then filtered through celite
6. concentrationconcentrated in high vacuum